Manufacture of sulfur, &amp;c.



- in a porc UNITED STATES PALIENT OFFICE.

HIPPOLYT KoHLER,

or BERLIN, GERMANY, nssreNon TO THE FIRM or RUTGERSWERKE AGTIENGESELLSGHAFT, or BERLIN, GERMANY.

Specification of Letters Patent.

Patented Sept. 8, 1908.

- Application filed May 18, 1907. Serial No. 374,467..-

To all whom it may concern:

Be it known that I, HIPPOLYT KoHLER, doctor of philosophy, chemist, a subject of the King of Bavaria and the German Emperor, residing at -3 Frobenstrasse, Berlin, German Empire, have invented new and useful Improvements in and Relating to the Manufacture of Sulfur Compounds, of which the following is a specification.

It is known that melted naphthalene is able to decompose sulfur (Lunge-Kohler, Industm'e des Steinlcohlenteers Fourth Edition Vol. 1 page 17 2). It hasnotliitherto been known, however, how a solution of sulfur in melted naphthalene behaves on cooling. At first it was thought that on coolin' the sulfur separated from the melted na ht h'alene in a pure crystalline condition. owever, it was shown that this natural assumption is not correct. On the cooling of the melted mass it is true that crystals are formed, but they do not consist of pure sulfur but are composed of naphthalene and sulfur, so that robably we have what is termed a fixed soution. It has proved to be possible to combine very considerable quantities of sulfur with naphthalene even at a temperature of from 85 to 90 C., which is only a few degrees above the melting point of naphthalene; that is to say 2 atoms of sulfur 64 parts by weight may be combined with 1 molecule of naphthalene 128 parts by weight. This molecular combination of naphthalene and sulfur also permits of absorbing still further quantities of naphthalene and sulfur. If such a liquid solution of 4 atoms of sulfur 128 arts by weight and 1 molecule of naphthaene. 128 arts by weight be allowed to cool e lain crucible which should however be rotected so that it does not cool too rapidly, until the surface of the liquid has set and the crust then broken and the still liquid contents allowed to flow out, it will be found that .the crucible is completely strewn with long pointed, highly lustrous crystals of a pale yellow color, which when washed with absolute alcohol, have a melting point of 98100-C. The mass when set also has the samemelting point. I

The crystals dlssolve readilyv in boiling benzol and crystals presenting the meltin oint of sulfur (113 to 115) are obtaine rom the solution. Decomposition therefore sets in and the benzol withdraws the melted naphthalene.

whole-of the napthalene from the product. I The same thing occurs on treating the reparation with alcohol; as, however, sul ur is not soluble in alcohol in this caseit separates out in a very finely divided condition. The napthalene also volatilizes gradually on exposure to the air, particular y with a moderate heat and leaves the sulfur behind likewise in a condition of the finestmolecular di-' Vision.

The property is also possessed to a high degree even by a product containing more than 4 molecules of sulfur, which, forv example, has been speedily cooled by vigorous stirring in cold. water. This ready decomposition of the product in question, and in'particular the circumstance that the sulfur is thereby separated out in an extremely finely divided condition, constitute a special feature. 4 molecules) presents approximately the hardness of ordinary sulfur and like this may The napthalene-sulfur (1 molecule:

be cast in rods or ground to the finest powder. lene-sulfur, to the known action of naphtha lene andalso to the sulfur present in a molec. ular condition, the product is specially suited for useas a deodorizer, disinfectant and antiparasitic (for example in the wine industry for combatting the oidium and phylloxera vastratrix (see Ernst Fischer, Berliner kl'i'n. Wochenschmft 1881 No. 48 and 1882 No. 8) for the manufacture of soaps, salves and the like, as a sulfur-yielding medium for chemical processes, say for example inthe Owing to these properties of naphtha vulcanization of caoutcho-uc, the manufac ture of wood cement and for-the production of molecular sulfur.

It cannot be definitely stated whether the described product is achemical ;oompound of naphthalene with sulfur or a so-called solid solution.

In manufacturing theproduct from naph-' thalene and sulfur, preferably the naphtha lene is melted and at a few degrees above its melting point (at 85 to 90) the coarsely pulverized sulfur is introduced into the It is advantageous to take equal quantities by weight of naphthalene andsulfur, but either one of the constituents may predominate in the mixture,

as the solubility of sulfur in naphthalene increases with the temperature. j It is, also possible, although less advantageous, to in troduce the naphthalene into the melted sulj fur. The final product may be poured into.

- sulfur may vided su molds and allowed to set, or cooled on metal surfaces in a thin layer, or (and this is most advanta eons for obtaining a very finely dilfur, particularly with a higher proportion than 4 molecules of sulfur to 1 molecule of naphthalene) it may be treated With agitating mechanism in cold water. The

also be converted into. a fine powder by rinding and sifting.

The ormation of the naphthalene sulfur may be also used for extracting sulfur from materials containing sulfur, for example from spent gas purifying masses. One brings fused naphthalene at or above the melting point of sulfur together with the mass to be extracted and se arates then the obtained naphthalene-Sn fur compound from the undissolvedmaterial for instance by decantating the fluid com ound, whereupon one may separate the nap thalene or use the formed com ound as above indicated.

What I 'c aim as my invention, and desire to secure by Letters Patent, is-

1. In the process of preparing finely divided sulfur, the ste which consists in fusingsulfur and naphtha ene together and allowing the fused mass to become solid.

2. Theprocess for preparing finely divided sulfur which consists in fusing sulfur and naphthalene together, allowing the fus'd mass to become solid and separating the naphthalene.

3. In the process of preparing finely divided sulfur, the step WhlOll consists in bringing fused naphthalene together with sulfur containing materials, and separating the formed naphthalene sulfur compound from the undissolved material.

In Witness whereof I have hereunto signed my name this 3rd day of May 1907', in the presence oftwo subscribing witnesses.

HIPPOLYT KCHLER.

Witnesses:

WOLDEMAR HAUPT, HENRY HAsrER. 

